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By leveraging the subtle refractive index evolution, including both the real and the imaginary parts, an entirely new concept of a lab\u2010on\u2010fiber operando method and its feasibility for \u201cpristine\u2010immersion\u2010operando\u2010post analysis\u201d of electrocatalyts are demonstrated. Concurrent collection of absorption spectra and surface plasmon resonance is achieved by engineering fiber\u2010optic waveguides\u00a0to simultaneously induce guided light attenuation and plasmonic coupling. In situ\u2010formed Co hydroxide and oxide reactive intermediates in zeolitic imidazolate framework\u201067 (ZIF\u201067) electrocatalyst are optically identified, which\u00a0shows its underlying self\u2010reconstruction conversions at different stages during electrocatalytic oxygen evolution reactions, and address the gap in knowledge concerning whether ZIF\u201067 is a precatalyst for real catalyst production. This illuminating operando method offers intriguing opportunities to collect all the observables in a single fiber, provides an exciting potential of a new class of device with long\u2010sought integration and miniaturization capability, and is expected to enable the electrocatalysis community to conquer challenges with conducting multimodal operando experiments outside the laboratory.<\/jats:p>","DOI":"10.1002\/adma.202411510","type":"journal-article","created":{"date-parts":[[2024,12,5]],"date-time":"2024-12-05T03:00:08Z","timestamp":1733367608000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":11,"title":["Lab\u2010on\u2010Fiber Operando Deciphering of a MOF Electrocatalyst"],"prefix":"10.1002","volume":"37","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-6679-3208","authenticated-orcid":false,"given":"Tiansheng","family":"Huang","sequence":"first","affiliation":[{"name":"Guangdong Provincial Key Laboratory of Optical 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